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Modified graphene and preparation method thereof

A graphene and modification technology, applied in the field of materials, can solve the problems of large specific surface area of ​​graphene, restricting the application of graphene, and thermodynamic instability, etc., achieving the effects of easy acquisition, easy satisfaction of operating conditions, and cost reduction

Inactive Publication Date: 2014-09-24
FUJIAN JIANGXIA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, graphene has a large specific surface area, high specific surface energy, and the van der Waals force between sheets is as high as 5.9 KJ mol-1, and is in a thermodynamically unstable state. Unless the graphene sheets are well separated, these factors It will lead to the irreversible agglomeration of graphene to form massive aggregates, and even to re-stack into graphite, thus losing its excellent properties
Undoubtedly, these problems severely restrict the application of graphene in concrete reinforcement and toughening.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A preparation method of modified graphene, specifically comprising the following steps:

[0038] 1) Add 500 g of 60-mesh natural flake graphite into 5 L of concentrated sulfuric acid at 0°C and stir for 2 h; then slowly add 225 g of potassium persulfate and 250 g of phosphorus pentoxide, stir for 3 h at 20°C, and then heat up to Stir at 40°C for 24 hours, then slowly add 20 L of water and stir for 2 hours, then slowly add 0.9 L of 30% hydrogen peroxide to obtain a suspension of bright yellow particles; separate the bright yellow particles by centrifugation, wash with water , dried in vacuum at 60°C for 12 h to obtain 486 g of graphene oxide;

[0039] 2) Add 480 g of graphene oxide into 4 L of thionyl chloride, reflux and stir at 80 °C for 24 h, then centrifuge, wash with acetone, and vacuum-dry at room temperature for 12 h to obtain Graphene 475 g;

[0040] 3) 470 g of graphene containing acid chloride groups on the surface and 305.5 g of 1,3-propanediamine were added...

Embodiment 2

[0044] A preparation method of modified graphene, specifically comprising the following steps:

[0045] 1) Add 1000 g of 100-mesh natural flake graphite to 10 L of concentrated sulfuric acid at 2°C and stir for 2 h; then slowly add 450 g of potassium persulfate and 500 g of phosphorus pentoxide, stir for 3 h at 23°C, and then heat up to Stir at 43°C for 24 hours, then slowly add 40 L of water and stir for 2 hours, then slowly add 1.8 L of 30% hydrogen peroxide to obtain a suspension of bright yellow particles; centrifuge the bright yellow particles, wash with water , dried under vacuum at 62°C for 16 h to obtain 990 g of graphene oxide;

[0046] 2) Add 985 g of graphene oxide into 7.88 L of thionyl chloride, reflux and stir at 80 °C for 28 h, then centrifuge, wash with acetone, and vacuum-dry at room temperature for 14 h to obtain Graphene 980 g;

[0047] 3) Add 980 g of graphene containing acid chloride groups on the surface and 637 g of 1,3-propanediamine to 4.2 L of N,N'-...

Embodiment 3

[0051] A preparation method of modified graphene, specifically comprising the following steps:

[0052] 1) Add 1500 g of 160-mesh natural flake graphite to 15 L of concentrated sulfuric acid at 0°C and stir for 3 h; then slowly add 675 g of potassium persulfate and 750 g of phosphorus pentoxide, stir for 4 h at 22°C, and then raise the temperature to Stir at 45°C for 36 h, then slowly add 60 L of water and stir for 3 h, then slowly add 2.7 L of 30% hydrogen peroxide to obtain a suspension of bright yellow particles; centrifuge the bright yellow particles and wash them with water , dried under vacuum at 65°C for 18 h to obtain 1475 g of graphene oxide;

[0053] 2) Add 1470 g of graphene oxide into 11.76 L of thionyl chloride, reflux and stir at 80 °C for 32 h, then centrifuge, wash with acetone, and vacuum-dry at room temperature for 16 h to obtain Graphene 1450g;

[0054] 3) 1450 g of graphene containing acid chloride groups on the surface and 942.5 g of 1,3-propanediamine w...

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Abstract

The invention discloses modified graphene and a preparation method thereof. The method comprises the following steps: performing oxidation treatment on natural flake graphite to obtain graphene oxide, and enabling graphene oxide to react with sulfoxide chloride to obtain graphene containing acyl chloride groups on the surface; then performing nucleophilic substitution reaction with 1,3-propane diamine, cyanuric chloride and a dihydric alcohol compound in sequence to obtain water-soluble graphene with hydroxyl groups on the surface, wherein the hydroxyl group content is 0.005-0.02%. Obtained modified graphene has relatively good water solubility, and is beneficial to stable dispersion of graphene; by adopting the characteristics of modified graphene, modified graphene can be mixed and uniformly dispersed with other concrete preparation materials very conveniently to prepare a reinforcing and toughening concrete product. In addition, operating conditions for preparing modified graphene can be easily met; moreover, modified graphene disclosed by the invention is easily-available in raw material, can be used for effectively reducing the cost and improving the economic benefits, and has relatively good application prospects.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a modified graphene and a preparation method thereof. Background technique [0002] Due to the complex and harsh stress environment of some building structures and parts in modern buildings, concrete with the highest possible strength and toughness must be used. In order to improve the strength and toughness of concrete products, carbon fiber, glass fiber, Futa fiber, steel wire / steel mesh fiber, polyvinyl alcohol fiber, polyester fiber, dura fiber, etc. have been used successively. [0003] In 2004, British scientist Geim A. K. and others discovered graphene, the super material with the highest strength and hardness. In just a few years, graphene surpassed the previously high-profile "superfiber" -- carbon nanotubes, and has become a global leader. A huge research upsurge has been set off in this field. Graphene can be regarded as single-layer graphite, and each ...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 蒋国平杜永峰郑敬云
Owner FUJIAN JIANGXIA UNIV
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